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WO2021225158A1 - Procédé de production de corps fritté en céramique, et corps fritté en céramique - Google Patents

Procédé de production de corps fritté en céramique, et corps fritté en céramique Download PDF

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Publication number
WO2021225158A1
WO2021225158A1 PCT/JP2021/017471 JP2021017471W WO2021225158A1 WO 2021225158 A1 WO2021225158 A1 WO 2021225158A1 JP 2021017471 W JP2021017471 W JP 2021017471W WO 2021225158 A1 WO2021225158 A1 WO 2021225158A1
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Prior art keywords
sintered body
condition
ceramic
mpa
heat treatment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/JP2021/017471
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English (en)
Japanese (ja)
Inventor
雄斗 大越
伸広 篠原
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AGC Inc
Original Assignee
Asahi Glass Co Ltd
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Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to CN202180032924.8A priority Critical patent/CN115551818A/zh
Priority to EP21800365.5A priority patent/EP4148031A4/fr
Priority to JP2022519630A priority patent/JPWO2021225158A1/ja
Publication of WO2021225158A1 publication Critical patent/WO2021225158A1/fr
Priority to US18/052,299 priority patent/US20230113344A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Definitions

  • the present invention relates to a method for producing a ceramic sintered body and a ceramic sintered body.
  • HIP Hot Isostatic Pressing
  • Patent Documents 1 to 3 describe that the HIP treatment is performed after increasing the density of the molded product by a CIP (Cold Isostatic Pressing) method in which an isotropic pressure is applied to the molded product in water. ..
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide a method for producing a ceramics sintered body and a ceramics sintered body capable of appropriately producing a dense ceramics sintered body.
  • the method for producing a ceramic sintered body according to the present disclosure includes a step of heat-treating a ceramic molded body, which is a molded body of ceramic powder, under the first condition, and the first.
  • the step of heat-treating the ceramic molded body heat-treated under the conditions under the second condition, which is higher than the first condition, and the step of heat-treating the ceramic molded body heat-treated under the second condition, the pressure of the ceramic molded body being higher than the second condition.
  • the ceramics sintered body according to the present disclosure is a spherical silicon nitride ceramics sintered body, and when the radius of the ceramics sintered body is r, fracture toughness value of the region of 1 / 10r from the surface of the ceramic sintered body (K IC) is not less 6.5 MPa ⁇ m 1/2 or more, fracture toughness of the region of 1 / 10r from the surface of the sintered ceramics
  • K IC fracture toughness value of the region of 1 / 10r from the surface of the ceramic sintered body
  • the difference ⁇ KA between the maximum value and the minimum value is 2.0 MPa ⁇ m 1/2 or less, and the maximum value and the minimum value of the fracture toughness value in the region of 1/10 r to 2/10 r of the ceramic sintered body.
  • the difference ⁇ KB is 1.5 MPa ⁇ m 1/2 or less.
  • a dense ceramic sintered body can be appropriately manufactured.
  • FIG. 1 is a flowchart illustrating a method for manufacturing a ceramic sintered body according to the present embodiment.
  • FIG. 2 is a flowchart illustrating the details of the process of producing the ceramic molded product.
  • FIG. 3 is a diagram showing a configuration example of the heat treatment furnace in the present embodiment.
  • FIG. 4 is a graph showing the fracture toughness value in Example 2.
  • FIG. 5 is a graph showing the fracture toughness value in Example 2.
  • the ceramic powder is molded to produce a ceramic molded body, and the ceramic molded body is fired to produce a ceramic sintered body.
  • the ceramic sintered body is a sintered body of silicon nitride (Si 3 N 4 ), and the ceramic powder is a silicon nitride powder.
  • the ceramic sintered body may contain silicon nitride as a main component and may contain a material other than silicon nitride, or may contain unavoidable impurities.
  • the content of silicon nitride with respect to the whole may be 80% or more, 83% or more, or 85% or more by weight.
  • the ceramic sintered body produced by this production method is used, for example, for a ball of a ball bearing (bearing ball, etc.), but the application is not limited to this and may be arbitrary.
  • the production method according to the present embodiment is for producing a sintered body of silicon nitride, but the method is not limited to silicon nitride and may be used for producing a sintered body of any ceramics. That is, the ceramic sintered body is not limited to silicon nitride and may be a sintered body made of any ceramics, and the ceramic powder may be a powder made of any ceramics, not limited to silicon nitride.
  • FIG. 1 is a flowchart for explaining a method for manufacturing a ceramic sintered body according to the present embodiment
  • FIG. 2 is a flowchart for explaining details of a process for producing a ceramic molded product.
  • the ceramic powder is molded to produce a ceramic molded body (step S10).
  • a ceramic molded product is produced by a gel casting method.
  • FIG. 2 shows details of an example of a step of producing a ceramic molded product by the gel casting method in step S10 of FIG.
  • a ceramic slurry is produced (step S10b).
  • the ceramic slurry is a slurry in which ceramic powder is dispersed in a solvent.
  • the method for producing the ceramic slurry is not particularly limited, and a dispersant, a sintering aid, a resin, and a resin curing agent may be appropriately added to the slurry containing the ceramic powder and the solvent depending on the type of the solvent and the like.
  • a ceramic powder, a solvent, a dispersant, and a sintering aid are mixed to obtain a slurry (hereinafter, also referred to as a raw ceramic slurry), and then a resin and a resin curing agent are added to the raw ceramic slurry. Is added to produce a ceramic slurry.
  • Ceramic powder is an essential component when performing a gel casting method.
  • the ceramic powder is, for example, silicon nitride, aluminum nitride, titanium nitride, or silicon carbide powder.
  • the solvent is an indispensable component when performing the gel casting method, and is a liquid for uniformly mixing and molding ceramic powder, sintering aid, resin and resin curing agent.
  • the solvent may be, for example, water, an organic solvent, or alcohols, as long as it does not remain in the ceramics sintered body after sintering.
  • alcohols for example, methyl alcohol and ethyl alcohol can be used.
  • organic solvent for example, benzene, toluene and xylene can be used. These solvents may be used alone or may be mixed as appropriate.
  • the dispersant is an additive that assists the dispersion of the ceramic powder in the solvent, and is an arbitrary component.
  • Dispersants include, for example, pH adjusters such as tetramethylammonium hydroxide, polymer dispersants such as polycarboxylic acid-type polymers, inorganic dispersants such as phosphates such as sodium hexametaphosphate, anions, and cations. It is a system-based or nonionic-based organic type surfactant type dispersant.
  • the sintering aid is an additive that assists in sintering ceramic powder, and is an arbitrary component.
  • the sintering aid when the ceramic powder is silicon nitride, the sintering aid includes magnesium oxide (MgO), aluminum oxide (Al 2 O 3 ), spinel (magnesia alumina spinel; MgO Al 2 O 3 ), and yttrium oxide (Y 2). O 3), may be used powder of a rare earth oxide such as ytterbium oxide (Yb 2 O 3).
  • a ball mill is used for pulverization and mixing, but the pulverization and mixing method may be arbitrary.
  • the amount of the ceramic powder added to the solvent is preferably 35% by volume or more and 65% by volume or less, more preferably 40% by volume or more and 60% by volume or less, and 45% by volume. It is more preferably 55% by volume or less.
  • the amount of the dispersant added to the ceramic powder is preferably 0.3% by weight or more and 3% by weight or less, and 0.4% by weight or more and 2% by weight or less. Is more preferable, and 0.5% by weight or more and 1% by weight or less is further preferable. With such a compounding ratio, a ceramic molded product can be appropriately produced.
  • the amount of the sintering aid added to the ceramic powder is preferably 1% by weight or more and 15% by weight or less, and more preferably 2% by weight or more and 12% by weight or less. It is preferably 3% by weight or more and 9% by weight or less. With such a compounding ratio, a ceramic sintered body can be appropriately manufactured.
  • a resin and a resin curing agent are added to the mixed raw ceramic slurry to generate a ceramic slurry (hereinafter, also referred to as a cast ceramic slurry) (step S10b). More specifically, a resin and a resin curing agent (polymerization initiator) are added to the raw material ceramic slurry.
  • the resin is a resin that polymerizes and cures when a resin curing agent is added, and in the present embodiment, it is preferable that the resin is a resin that dissolves in the solvent of the ceramic slurry (here, a water-soluble resin).
  • the resin here is, for example, a water-soluble epoxy resin, but is not limited to the epoxy resin, and may be any resin that polymerizes and cures by adding a resin curing agent.
  • a resin curing agent is an additive that polymerizes and cures a resin by being added to the resin.
  • the resin curing agent here is, for example, a mixture of triethylenetetramine and dimethylaminomethyl, but is not limited to this, and may be any additive that polymerizes and cures the resin by being added to the resin. ..
  • a resin-added ceramic slurry in which a resin is added to a raw material ceramic slurry (hereinafter, also referred to as a first ceramic slurry) and a curing agent-added ceramic slurry in which a resin curing agent is added to a raw material ceramic slurry (hereinafter, referred to as a second ceramics slurry).
  • a first ceramic slurry a raw material ceramic slurry
  • a curing agent-added ceramic slurry in which a resin curing agent is added to a raw material ceramic slurry hereinafter, referred to as a second ceramics slurry
  • the amount of the resin added to the ceramic powder in the ceramic slurry is preferably 1% by weight or more and 10% by weight or less, and more preferably 1.5% by weight or more and 8% by weight or less. It is more preferable that the content is 2% by weight or more and 5% by weight or less. With such a compounding ratio, a ceramic molded product can be appropriately produced. Further, the amount of the resin curing agent added to the resin is preferably an amount that is stoichiometrically appropriate for the added resin. With such a compounding ratio, a ceramic molded product can be appropriately produced.
  • the cast ceramic slurry is injected into the molding mold (step S10c).
  • the resin and the resin curing agent are separately added to the raw ceramic slurry and then mixed, that is, the first ceramic slurry and the second ceramic slurry are separately generated and mixed.
  • both the resin and the resin curing agent may be added to the raw material ceramic slurry, and the cast ceramic slurry to which both are added may be injected into the molding die.
  • the ceramic slurry is held at a predetermined holding temperature for a predetermined holding time in a state of being supplied to the molding die.
  • the holding temperature here is preferably 25 ° C. or higher and 100 ° C. or lower, more preferably 30 ° C. or higher and 80 ° C. or lower, and further preferably 40 ° C. or higher and 60 ° C. or lower.
  • the holding time here is preferably 1 hour or more and 48 hours or less, more preferably 2 hours or more and 24 hours or less, and further preferably 3 hours or more and 12 hours or less.
  • a pressure higher than the atmospheric pressure may be applied to the ceramic slurry.
  • the cured product obtained by curing the ceramic slurry is removed from the mold (taken out), and the cured product is appropriately dried and degreased to obtain a ceramic molded product (step S10d).
  • the demolded cured product is dried to obtain a dry molded product, and the dry molded product is degreased to obtain a ceramic molded product.
  • the drying conditions are arbitrary, but for example, a humidification drying treatment and a hot air drying treatment are performed. In the humidifying and drying treatment, the cured product is held for 24 hours or more and 120 hours or less in an environment where the humidity is 30% or more and 98% or less and the temperature is 25 ° C. or more and 50 ° C. or less.
  • the cured product is held for 3 hours or more and 48 hours or less while blowing air on the cured product in an environment where the temperature is 40 ° C. or higher and 100 ° C. or lower to obtain a dry molded product.
  • the degreasing method is also arbitrary, but for example, the dry molded product is held for 2 hours or more and 12 hours or less in an environment where the temperature is 550 ° C. or higher and 750 ° C. or lower, and degreased to obtain a ceramic molded product.
  • drying is a process of removing the solvent in the cured product
  • degreasing is a process of removing the resin in the cured product (dry molded product). Insufficient removal of these causes cracks during the firing process, which is an essential process in the gel casting method.
  • the ceramic molded product molded by this production method preferably has a relative density of 40% or more, more preferably 45% or more, and further preferably 50% or more.
  • the relative density is preferably high, but it may be 65% or less, 60% or less, or 55% or less.
  • the relative density here refers to a value obtained by dividing the molded product density by the substance density.
  • the molded body density is a value obtained by dividing the volume obtained from the dimensions of the ceramic molded body by the weight of the ceramic molded body.
  • the substance density is calculated from the composition ratio of the ceramic powder and the sintering aid and the theoretical density of each substance.
  • the material densities are, for example, ceramic powder (molar mass ag / mol, theoretical density Ag / cm 3 ) and sintering aid (molar mass pg / mol, theoretical density Bg / cm 3 ), X mol% and Y mol, respectively.
  • ceramic powder molecular weight ag / mol, theoretical density Ag / cm 3
  • sintering aid molecular weight pg / mol, theoretical density Bg / cm 3
  • the ceramic molded product is prepared by using the gel casting method as described above.
  • the method for producing the ceramic molded product is not limited to the gel casting method, and may be any method.
  • a powder pressing method may be used in which the ceramic powder filled in the molding die is pressed to form the ceramic molded body.
  • the ceramics sintered body is subjected to at least three stages of heat treatment, that is, heat treatment under the first condition, heat treatment under the second condition, and heat treatment under the third condition.
  • the heat treatment here refers to a process of heating an object at a temperature equal to or higher than a temperature at which at least a part of the ceramic powder starts sintering, and does not include a process at room temperature such as a CIP process.
  • the heat treatment under the first condition, the heat treatment under the second condition, and the heat treatment under the third condition are performed in three stages, but the heat treatment is not limited to this, and the heat treatment in four or more stages is performed. It may be carried out.
  • the ceramic molded product dry molded product
  • the ceramic molded product may be subjected to CIP treatment before the heat treatment. By the CIP treatment, pressure can be applied isotropically to the ceramic molded product, and the relative density of the molded product can be increased.
  • the heat treatment under the first condition will be described.
  • the ceramic molded product is heat-treated under the first condition (step S12).
  • the temperature for heating the ceramic molded body is defined as the first heating temperature
  • the pressure applied to the ceramic molded body is defined as the first pressure
  • the heating time is defined as the first heating time.
  • the first condition that is, the first heating temperature, the first pressure, and the first heating time depends on the properties of the ceramic powder, the amount and type of the sintering aid added, the relative density, shape, and dimensions of the ceramic molded body. , May be set as appropriate.
  • the first heating temperature is preferably 1600 ° C. or higher and 1800 ° C. or lower, more preferably 1620 ° C. or higher and 1780 ° C. or lower, and further preferably 1650 ° C. or higher and 1750 ° C. or lower. ..
  • the first pressure is preferably 0.01 MPa or more and 5 MPa or less, more preferably 0.05 MPa or more and 3 MPa or less, and further preferably 0.1 MPa or more and 1 MPa or less. By setting the first pressure in this range, the relative density of the sintered body can be set in an appropriate range.
  • the heat treatment under the first condition is most preferably performed at normal pressure (atmospheric pressure), that is, 0.1 MPa from the viewpoint of mass productivity and operability.
  • the first heating time is preferably 1 hour or more and 20 hours or less, more preferably 2 hours or more and 18 hours or less, and further preferably 5 hours or more and 15 hours or less. By setting the first heating time in this range, the relative density of the sintered body can be set in an appropriate range.
  • the heat treatment under the first condition is performed in a nitrogen atmosphere.
  • the sintering of the ceramic powder which is silicon nitride, can be appropriately performed.
  • the ceramic molded body is subjected to the heat treatment under the first condition in this way, so that it is first sintered, that is, primary sintered.
  • first sintered that is, primary sintered.
  • the relative density of the first sintered body is preferably 85% or more, preferably 90% or more. More preferably, it is more preferably 95% or more.
  • the relative density is obtained by dividing the density of the first sintered body measured according to JIS R 1634 by the substance density calculated from the composition ratio of the ceramic powder and the sintering aid and the theoretical density of each substance. Value.
  • the heat treatment under the second condition is a heat treatment under a high pressure environment more than the heat treatment under the first condition, and can be said to be a GPS (Gas Pressure Sintering) treatment.
  • the temperature for heating the first sintered body is defined as the second heating temperature
  • the pressure applied to the first sintered body is defined as the second pressure
  • the heating time is defined as the second heating time. ..
  • the second heating temperature is preferably higher than the first heating temperature under the first condition, but may be a temperature equal to or lower than the first heating temperature.
  • the second heating temperature is preferably 1650 ° C. or higher and 1900 ° C. or lower, more preferably 1680 ° C. or higher and 1850 ° C. or lower, and further preferably 1700 ° C. or higher and 1800 ° C. or lower.
  • the second pressure is higher than the first pressure in the heat treatment under the first condition.
  • the difference between the second pressure and the first pressure is preferably 0.3 MPa or more and 20 MPa or less, more preferably 1 MPa or more and 18 MPa or less, and further preferably 2 MPa or more and 15 MPa or less.
  • the second pressure is preferably 0.5 MPa or more and 20 MPa or less, more preferably 3 MPa or more and 18 MPa or less, and further preferably 5 MPa or more and 15 MPa or less.
  • the second heating time is preferably shorter than the first heating time.
  • the second heating time is preferably 0.1 hour or more and 10 hours or less, more preferably 0.15 hours or more and 8 hours or less, and further preferably 0.2 hours or more and 6 hours or less.
  • the heat treatment under the second condition is performed in a nitrogen atmosphere.
  • the sintering of the ceramic powder which is silicon nitride, can be appropriately performed.
  • the heat treatment under the second condition may be performed after the heat treatment under the first condition is completed, the first sintered body is taken out and cooled, or the heat treatment under the first condition is performed after the first sintering. It may be performed continuously without cooling the body.
  • the first sintered body is subjected to the heat treatment under the second condition in this way, so that it is second-sintered, that is, second-sintered. It is considered that the heat treatment under the second condition, which is higher than the first condition, reduces the fine pores on the surface of the sintered body and makes the surface denser. It is possible to effectively carry out the heat treatment under the third condition by suppressing the gas from penetrating into the sintered body.
  • the ceramic molded product that has been heat-treated under the second condition that is, the first sintered body that has been heat-treated under the second condition is the second sintered body
  • the second sintered body The relative density is preferably 95% or more, more preferably 97% or more.
  • the relative density of the second sintered body is preferably high, but may be 99% or less.
  • the heat treatment under the third condition is performed on the ceramic molded body heat-treated under the second condition, that is, the second sintered body.
  • Step S16 a ceramic sintered body is produced.
  • the heat treatment under the third condition is a heat treatment under a high pressure environment more than the heat treatment under the second condition, and can be said to be a HIP treatment.
  • the temperature for heating the second sintered body is defined as the third heating temperature
  • the pressure applied to the second sintered body is defined as the third pressure
  • the heating time is defined as the third heating time. ..
  • the third heating temperature is preferably higher than the first heating temperature under the first condition, but may be a temperature equal to or lower than the first heating temperature. Further, the third heating temperature may be higher than the second heating temperature under the second condition, or may be a temperature equal to or lower than the second heating temperature.
  • the third heating temperature is preferably 1650 ° C. or higher and 1900 ° C. or lower, more preferably 1680 ° C. or higher and 1850 ° C. or lower, and further preferably 1700 ° C. or higher and 1800 ° C. or lower. By setting the third heating temperature in this range, the relative density of the ceramic sintered body can be set to an appropriate value. Further, the third pressure is higher than the second pressure in the heat treatment under the second condition.
  • the difference between the third pressure and the second pressure is preferably 30 MPa or more and 180 MPa or less, more preferably 40 MPa or more and 160 MPa or less, and further preferably 50 MPa or more and 130 MPa or less.
  • the third pressure is preferably 50 MPa or more and 200 MPa or less, more preferably 60 MPa or more and 180 MPa or less, and further preferably 70 MPa or more and 150 MPa or less. By setting the third pressure in this range, the relative density of the ceramic sintered body can be set to an appropriate value.
  • the third heating time is preferably 0.1 hour or more and 10 hours or less, more preferably 0.15 hours or more and 8 hours or less, and further preferably 0.2 hours or more and 6 hours or less. By setting the third heating time in this range, the relative density of the ceramic sintered body can be set to an appropriate value.
  • the heat treatment under the third condition is performed in a nitrogen atmosphere.
  • the sintering of the ceramic powder which is silicon nitride, can be appropriately performed.
  • the heat treatment under the third condition may be performed after the heat treatment under the second condition is completed, the second sintered body is taken out and cooled, or the heat treatment under the second condition is performed after the second sintering. It may be performed continuously without cooling the body.
  • the second sintered body is subjected to the heat treatment under the third condition in this way, so that it is sintered for the third time, that is, tertiary sintered.
  • the HIP treatment is performed without performing the CIP treatment.
  • the ceramic sintered body after the heat treatment under the third condition preferably has a relative density of 99% or more. By setting the relative density within this range, the performance of the ceramic sintered body can be guaranteed.
  • the ceramic sintered body preferably has a three-point bending strength of 900 MPa or more, more preferably 910 MPa or more, and 915 MPa or more at a span of 30 mm measured by the method specified by JIS R 1669. Is more preferable. When the three-point bending strength is within this range, the strength of the ceramic sintered body can be appropriately maintained. Further, the ceramic sintered body preferably has a fracture toughness value of 5.0 MPa ⁇ m 1/2 or more and 5.5 MPa ⁇ m 1/2 or more measured by the method specified by JIS R 1669. Is more preferable, and 6.0 MPa ⁇ m 1/2 or more is further preferable.
  • the fracture toughness value is within this range, the strength of the ceramic sintered body can be appropriately maintained.
  • the number of pores of 5 ⁇ m or more observed using an optical microscope for an area of 1 mm 2 or more on a surface with an arbitrary cross section polished is 20 or less per 1 mm 2 area. It is preferable that the number is 15, more preferably 15 or less, and further preferably 10 or less.
  • the ceramic sintered body preferably has a maximum pore diameter of 25 ⁇ m or less, more preferably 15 ⁇ m or less, and further preferably 10 ⁇ m or less. When the number of pores and the maximum diameter are within this range, the performance of the ceramic sintered body can be guaranteed.
  • the ceramic sintered body is a silicon nitride sintered body, and is preferably spherical.
  • the sphere here is not limited to a sphere, and may be, for example, a sphericity of preferably within 3%, more preferably within 2.5%, and even more preferably within 2% with respect to the diameter.
  • the sphericity is preferably 1.5 mm or less, more preferably 1.25 mm or less, and even more preferably 1.0 mm or less.
  • the sphericity is preferably 0.3 mm or less, more preferably 0.25 mm or less, and even more preferably 0.2 mm or less.
  • the diameter of the ceramic sintered body is preferably 0.5 mm or more and 80 mm or less, more preferably 30 mm or more and 55 mm or less, and further preferably 49 mm or more and 51 mm or less. When the diameter is in this range, it can be suitably used for, for example, a bearing ball.
  • the diameter here may refer to an average diameter (arithmetic mean value of the maximum value and the minimum value of the diameter).
  • the radius of the ceramic sintered body will be r.
  • the radius r may be a value that is half the diameter of the ceramic sintered body.
  • Ceramic sintered body, fracture toughness value in the region (range) from the surface to a depth r / 10 (K IC) is preferably at 6.5 MPa ⁇ m 1/2 or more.
  • the difference ⁇ KA between the maximum value and the minimum value of the fracture toughness value in the range from the surface to the depth r / 10 is preferably 2.0 MPa ⁇ m 1/2 or less, preferably 1.5 MPa. - more preferably m 1/2 or less, and more preferably 1.2 MPa ⁇ m 1/2 or less.
  • the ceramic sintered body has a difference ⁇ KB between the maximum value and the minimum value of the fracture toughness value in the range from the position of the depth r / 10 from the surface to the depth 2r / 10 from the surface of 1.5 MPa ⁇ m 1. It is preferably / 2 or less, more preferably 1.0 MPa ⁇ m 1/2 or less, and further preferably 0.7 MPa ⁇ m 1/2 or less.
  • the fracture toughness value in the range from the surface to the depth r / 10 is in this range, the falling off of particles due to microscopic fracture can be suppressed, and the wear of the ceramic sintered body can be suppressed.
  • the ceramic sintered body according to the present embodiment has a high fracture toughness value particularly in the vicinity of the surface, and the fracture toughness value does not fluctuate up and down. Therefore, the ceramics sintered body has improved wear resistance, and for example, a ceramics sintered body having excellent sliding characteristics can be provided.
  • the fracture toughness value in the range from the surface to the depth r / 10 and the fracture toughness value in the range from the position of the depth r / 10 from the surface to the depth 2r / 10 from the surface are ceramic sintering. It is obtained by cutting the body into a disk so as to pass through the diameter, polishing one of the cut surfaces, and measuring the fracture toughness value at each position along the radial direction of the sphere. That is, for example, the fracture toughness value in the range from the surface to the depth r / 10 refers to the fracture toughness value in the region from the peripheral edge to a position r / 10 away from the peripheral edge on the central side of the cut surface. ..
  • the fracture toughness value can be measured using the Vickers hardness test system ARS9000 manufactured by Future Tech Co., Ltd. under the conditions of a load of 5 kg and a pushing time of 15 seconds.
  • the method for measuring the fracture toughness value may be the same thereafter.
  • the range from the surface to the depth r / 10 of the ceramic sintered body can be rephrased as, for example, the range from the surface to 2.5 mm. Further, the range from the position of the ceramic sintered body at a depth of r / 10 to the depth of 2r / 10 of the surface is from a position 2.5 mm deeper than the surface to 5.0 mm deeper than the surface. It can be rephrased as the range to the position.
  • the ceramic sintered body preferably has a fracture toughness value of 6.5 MPa ⁇ m 1/2 or more in the range from the surface to a depth of 2r / 10.
  • the fracture toughness value in the range from the surface to the depth of 2r / 10 is in this range, the falling off of particles due to microscopic fracture can be suppressed, and the wear of the ceramic sintered body can be more preferably suppressed.
  • the range of the ceramic sintered body from the surface to the depth of 2r / 10 can be rephrased as, for example, the range from the surface to 5.0 mm.
  • the ceramic sintered body preferably has an average fracture toughness value of 7.0 MPa ⁇ m 1/2 or more in the range from the surface to a depth of 4 r / 10.
  • the range of the ceramic sintered body from the surface to the depth of 4r / 10 can be rephrased as, for example, the range from the surface to 10.0 mm.
  • the standard deviation of the fracture toughness value in the range from the surface to the depth r / 10 is preferably 0.70 or less, more preferably 0.60 or less, and 0.40 or less. Is more preferable.
  • the standard deviation of the fracture toughness value in the range from the surface to the depth r / 10 within this range, the variation in the fracture toughness value is small, the ceramic sintered body becomes dense, and the non-uniformity of particles is suppressed. Wear of the ceramic sintered body can be suppressed more preferably.
  • the standard deviation of the fracture toughness value in the range from the surface to the depth of 4r / 10 is preferably 0.55 or less, more preferably 0.50 or less, and 0.48 or less. Is more preferable.
  • the standard deviation of the fracture toughness value in the range from the surface to the depth of 4r / 10 within this range, the variation in the fracture toughness value is small, the ceramic sintered body becomes dense, and the non-uniformity of particles is suppressed. Wear of the ceramic sintered body can be suppressed more preferably.
  • the ceramic sintered body preferably has a Vickers hardness in the range from the surface to a depth of 2r / 10 of 10 HV or more, more preferably 12 HV or more, and further preferably 14 HV or more.
  • the Vickers hardness in the range from the surface to the depth of 2r / 10 is determined by cutting the ceramic sintered body into a disk so as to pass through the diameter, and then polishing one of the cut surfaces along the radial direction of the sphere.
  • the fracture toughness value in the range from the surface to the depth of 2r / 10 refers to the Vickers hardness in the region of the cut surface from the peripheral edge to a position 2r / 10 away from the peripheral edge on the central side.
  • the Vickers hardness can be measured using the Vickers hardness test system ARS9000 manufactured by Future Tech Co., Ltd. under the conditions of a load of 5 kg and a pushing time of 15 seconds.
  • the ceramic sintered body according to the present embodiment is manufactured by the manufacturing method described in the present embodiment, but the manufacturing method may be arbitrary as long as it has the characteristics described above.
  • FIG. 3 is a diagram showing a configuration example of the heat treatment furnace in the present embodiment.
  • the heat treatment furnace 10 shown in FIG. 3 may be used to perform the heat treatment under the third condition, that is, the HIP treatment.
  • the heat treatment furnace 10 is a furnace capable of HIP processing.
  • the heat treatment furnace 10 includes a container 12, a base 14, a heating unit 16, and a heat insulating unit 18.
  • the base 14 is a base on which the second sintered body A, which is the object to be heat-treated, is installed.
  • the heating unit 16 is a heater arranged around the space where the second sintered body on the base 14 is installed, and heats the second sintered body A on the base 14.
  • the heat insulating portion 18 is a member that covers the heating portion 16 and the space on the base 14 where the second sintered body A is installed.
  • the heat insulating portion 18 is made of a member having a high heat insulating property, and insulates the internal space with respect to the external space.
  • the container 12 is a container for accommodating the base 14, the heating portion 16, and the heat insulating portion 18.
  • a gas introduction port 12a is formed in the container 12.
  • the heat treatment furnace 10 may be used for the heat treatment under the first condition, or may be used for the heat treatment under the second condition. By using the same heat treatment furnace 10, the heat treatment under the first condition, the heat treatment under the second condition, and the heat treatment under the third condition can be continuously performed.
  • the configuration of the heat treatment furnace 10 is an example, and in this manufacturing method, the heat treatment under the first condition, the heat treatment under the second condition, and the heat treatment under the third condition may be performed by using any equipment. ..
  • the method for producing the ceramic sintered body according to the present embodiment includes a step of heat-treating the ceramic molded body, which is a molded body of ceramic powder, under the first condition, and a ceramic molded body heat-treated under the first condition.
  • the step of heat-treating the (first sintered body) under the second condition, which is higher than the first condition, and the ceramic molded body (second sintered body) heat-treated under the second condition are more than those of the second condition. It includes a step of producing a ceramics sintered body by heat treatment under a third condition of high pressure.
  • the heat treatment is carried out stepwise while increasing the pressure under the first condition, the second condition and the third condition, the pores are sufficiently removed to obtain high strength, and the dense ceramic sintered body is obtained. Can be properly manufactured.
  • the high-pressure gas may permeate into the pores, and firing may not be performed properly.
  • the present manufacturing method by increasing the pressure stepwise and performing the heat treatment, it is possible to appropriately remove air bubbles and appropriately perform the high pressure heat treatment.
  • CIP treatment before high-pressure heat treatment becomes unnecessary.
  • the work load may increase because the molded body needs to be sealed with a rubber mold or the like so as not to be flooded, and it is difficult to cope with a complicated shape.
  • the CIP process if the CIP process is not executed, the HIP process cannot be appropriately executed, and there is a risk that a dense sintered body cannot be produced.
  • the present manufacturing method since the heat treatment is carried out stepwise while increasing the pressure under the first condition, the second condition and the third condition, the high pressure HIP treatment is appropriately performed without performing the CIP treatment. Therefore, it is possible to manufacture a dense ceramic sintered body having a complicated shape while reducing the work load.
  • the difference between the second pressure applied to the ceramic molded body in the step of heat-treating under the second condition and the first pressure applied to the ceramic molded body in the step of heat-treating under the first condition is set to 0. It is preferable that the pressure is 3 MPa or more and 20 MPa or less, and the difference between the third pressure applied to the ceramic molded body and the second pressure in the step of heat treatment under the third condition is 30 MPa or more and 180 MPa or less.
  • the first pressure applied to the ceramic molded body in the step of heat-treating under the first condition is set to 0.01 MPa or more and 5 MPa or less, and the ceramic molded body (first firing) in the step of heat-treating under the second condition. It is preferable that the pressure applied to the body) is 0.5 MPa or more and 20 MPa or less, and the pressure applied to the ceramic molded body (second sintered body) in the step of heat treatment under the third condition is 50 MPa or more and 200 MPa or less. .. By setting each pressure in this range, it is possible to appropriately carry out stepwise heat treatment while increasing the pressure to appropriately produce a dense ceramic sintered body.
  • the heat treatment temperature under the first condition is set to 1600 ° C. or higher and 1800 ° C. or lower
  • the heat treatment temperature under the second condition is set to 1700 ° C.
  • the temperature is 1900 ° C. or lower
  • the heat treatment temperature under the third condition is 1700 ° C. or higher and 1900 ° C. or lower.
  • this production method it is preferable to further include a step of molding ceramic powder by a gel casting method to produce a ceramic molded product.
  • a ceramic molded product can be appropriately produced.
  • even a ceramic molded body having a complicated shape can be easily manufactured.
  • the ceramic sintered body is preferably a silicon nitride sintered body. According to this production method, a dense sintered body of silicon nitride can be appropriately produced.
  • the step of heat-treating under the first condition, the second condition, and the third condition it is preferable to heat-treat the ceramic molded product in a nitrogen atmosphere.
  • a dense sintered silicon nitride can be appropriately produced.
  • the ceramic sintered body produced by heat treatment under the third condition has a three-point bending strength of 900 MPa or more at a span of 30 mm measured by the method specified by JIS R 1669, and is the method specified by JIS R 1669.
  • the fracture toughness value measured in 1 is 5.0 MPa ⁇ m 1/2 or more, and the number of pores of 5 ⁇ m or more observed using an optical microscope for an area of 1 mm 2 or more on a surface with an arbitrary cross section polished. However, it is preferable that the number is 10 or less per 1 mm 2 area, and the maximum diameter of the pores is 10 ⁇ m or less. According to this manufacturing method, a high-performance ceramics sintered body can be provided by manufacturing a ceramics sintered body having such characteristics.
  • Example 1 Next, Example 1 will be described. Table 1 shows the production conditions of the ceramics sintered body according to each example and the evaluation results of the manufactured ceramics sintered body.
  • Example 1 silicon nitride powder as a ceramic powder (manufactured by Denka: SN-9FWS), spinel powder as a sintering aid, ion-exchanged water as a solvent, and tetramethylammonium hydroxide as a dispersant.
  • SN-9FWS silicon nitride powder as a ceramic powder
  • spinel powder as a sintering aid
  • ion-exchanged water as a solvent
  • tetramethylammonium hydroxide as a dispersant.
  • a water-soluble epoxy resin manufactured by Nagase ChemteX: EX614B, EX512
  • a resin is added to a part of the silicon nitride slurry and mixed to generate a first ceramics slurry, and the other part of the silicon nitride slurry is produced.
  • a mixture of triethylenetetramine as a resin curing agent and dimethylaminomethyl at a mass ratio of 2: 1 was added and mixed to generate a second ceramic slurry.
  • the first ceramic slurry and the second ceramic slurry are defoamed by reducing the pressure in individual tanks, and while being stirred in the tank, they are simultaneously sent to a mixing mixer to be mixed and cast ceramic slurry. And supplied to the molding die connected to the mixer outlet. Then, the mold filled with the ceramic slurry (mixture of the first ceramic slurry and the second ceramic slurry) was held at 50 ° C. for 5 hours to cure the ceramic slurry to obtain a cured product. Then, the cured product was removed from the mold, humidified and dried at 30 ° C. for 4 days, and then dried with hot air at 50 ° C. to obtain a dry molded product. Then, the dry molded product was heated at 600 ° C.
  • the density and relative density of the obtained ceramic molded product were measured.
  • the value obtained by dividing the volume obtained from the dimensions of the ceramic molded body by the weight of the ceramic molded body is taken as the molded body density, and from the composition ratio of the ceramic powder and the sintering aid and the theoretical density of each substance.
  • the value obtained by dividing the molded body density by the material density was taken as the relative density.
  • the material densities are, for example, silicon nitride (theoretical density 3.18 g / cm 3 ) as a ceramic powder and magnesia alumina spinel (theoretical density 3.6 g / cm 3 ) as a sintering aid, 95 mol% and 5 mol, respectively. when mixed with% composition ratio, the volume of 100g is 31.26Cm 3, material density becomes 3.20 g / cm 3.
  • the ceramic molded product was not subjected to CIP treatment. Then, as the heat treatment under the first condition, the ceramic molded body was heat-treated at 1600 ° C. for 10 hours in a nitrogen atmosphere at a pressure of 0.1 MPa to obtain a first sintered body.
  • the sintered body density and the relative density were measured with respect to the obtained first sintered body.
  • Sintered body density was measured according to JIS R 1634.
  • the relative density was defined as the material density calculated from the composition ratio of the ceramic powder and the sintering aid and the theoretical density of each substance, and the value obtained by dividing the sintered body density by the material density was defined as the relative density.
  • the first sintered body was heat-treated at 1700 ° C. for 1.5 hours in a nitrogen atmosphere at a pressure of 10 MPa as a heat treatment under the second condition to obtain a second sintered body.
  • the sintered body density and the relative density were measured with respect to the obtained second sintered body.
  • the second sintered body was heat-treated at 1750 ° C.
  • the density, the average strength, the pore frequency, the average pore diameter, and the maximum pore diameter were measured.
  • the average strength was measured with an autocom type universal testing machine (AC-100KN-C manufactured by TSE Co., Ltd.).
  • the pore frequency refers to the number of pores of 5 ⁇ m or more observed using an optical microscope with respect to an area of 1 mm 2 or more on the polished surface of the ceramic sintered body per 1 mm 2 area.
  • the average pore diameter was measured with an industrial microscope (LV100 manufactured by Nikon Corporation).
  • the maximum pore diameter was measured with an industrial microscope (LV100 manufactured by Nikon Corporation).
  • Example 2 a ceramic sintered body was produced by the same method as in Example 1 except that the Sp amount was 4 mol% and the heat treatment under the first condition was performed at 1700 ° C. for 5 hours.
  • Example 3 a ceramic sintered body was produced by the same method as in Example 2.
  • Example 4 a ceramic sintered body was produced by the same method as in Example 1 except that the Sp amount was 4 mol%.
  • Example 5 In Example 5, the Sp amount was 4 mol%, and the heat treatment under the first condition was performed at 1600 ° C. for 5 hours to obtain a first sintered body. Then, the first sintered body was heat-treated at 1800 ° C. for 5 hours in a nitrogen atmosphere at a pressure of 0.8 MPa as a heat treatment under the second condition to obtain a second sintered body. Then, as the heat treatment under the third condition, the second sintered body was heat-treated at 1750 ° C. for 2 hours in a nitrogen atmosphere at a pressure of 100 MPa to obtain a ceramic sintered body.
  • Example 6 the ceramic sintered body was produced by the same method as in Example 1 except that the Sp amount was 4 mol% and the ceramic molded body was subjected to CIP treatment.
  • Example 7 the ceramics sintered body was produced by the same method as in Example 1 except that the ceramic molded body was subjected to CIP treatment and the heat treatment under the second condition was set at 1800 ° C. for 0.25 hours.
  • Example 8 the ceramic sintered body was manufactured by the same method as in Example 1 except that the Sp amount was 4 mol%, the ceramic molded body was subjected to CIP treatment, and the heat treatment under the second condition was not performed. ..
  • Example 9 a ceramic sintered body was produced in the same manner as in Example 8.
  • Example 10 is the same method as in Example 1 except that the ceramic compact is CIP-treated, the heat treatment under the first condition is performed at 1730 ° C. for 3 hours, and the heat treatment under the second condition is not performed. A sintered body was manufactured.
  • Example 11 a ceramic sintered body was produced by the same method as in Example 1 except that the Sp amount was 4 mol% and the heat treatment under the second condition was not performed.
  • Example 12 In Example 12, the Sp amount was 4 mol%, the heat treatment under the first condition was set at 1700 ° C. for 5 hours, and the ceramic baking was performed by the same method as in Example 1 except that the heat treatment under the second condition was not performed. Manufactured the body.
  • Example 13 In Example 13, a ceramic sintered body was produced in the same manner as in Example 12.
  • Example 14 In Example 14, the Sp amount was 4 mol%, the heat treatment under the first condition was set at 1700 ° C. for 5 hours, the heat treatment under the second condition was not carried out, and the heat treatment under the third condition was set at 1750 ° C. for 5 hours.
  • a ceramic sintered body was produced by the same method as in Example 1 except for the points.
  • Example 15 In Example 15, a ceramic sintered body was produced in the same manner as in Example 14.
  • Example 16 In Example 16, the Sp amount was 4 mol%, the heat treatment under the first condition was performed at 1700 ° C. for 5 hours, the heat treatment under the second condition was not performed, and the heat treatment under the third condition was performed at 1800 ° C. for 2 hours.
  • a ceramic sintered body was produced by the same method as in Example 1 except for the above points.
  • Example 17 is the same as Example 1 except that the heat treatment under the first condition is performed at 1700 ° C. for 15 hours, the heat treatment under the second condition is performed at 1700 ° C. for 1 hour, and the heat treatment under the third condition is not performed.
  • a ceramic sintered body was produced by the method.
  • Example 18 In Example 18, a ceramic sintered body was produced in the same manner as in Example 17.
  • Example 19 In Example 19, the Sp amount was 4 mol%, the heat treatment under the first condition was 1700 ° C. for 15 hours, the heat treatment time under the second condition was 2 hours, and the heat treatment time under the third condition was 5 hours.
  • the Sp amount was 4 mol%
  • the heat treatment under the first condition was 1700 ° C. for 15 hours
  • the heat treatment time under the second condition was 2 hours
  • the heat treatment time under the third condition was 5 hours.
  • Example 20 In Example 20, the Sp amount was 4 mol%, the heat treatment under the first condition was 1700 ° C. for 5 hours, the heat treatment time under the second condition was 2 hours, and the heat treatment time under the third condition was 5 hours.
  • the Sp amount was 4 mol%
  • the heat treatment under the first condition was 1700 ° C. for 5 hours
  • the heat treatment time under the second condition was 2 hours
  • the heat treatment time under the third condition was 5 hours.
  • a ceramic sintered body having a density of 3.15 g / cm 3 or more was regarded as acceptable, and a ceramic sintered body having a density of less than 3.15 g / cm 3 was evaluated as rejected. Further, when the average strength of the ceramic sintered body was 900 MPa or more, it was regarded as acceptable, and when it was less than 900 MPa, it was rejected. Further, the ceramic sintered body having a pore frequency of 10 or less was regarded as acceptable, and the ceramic sintered body having a pore frequency greater than 10 was regarded as rejected.
  • the ceramic sintered body having an average pore diameter of 6.4 ⁇ m or less was regarded as acceptable, and the ceramic sintered body having a pore average diameter of larger than 6.4 ⁇ m was rejected. Further, a ceramic sintered body having a maximum pore diameter of 10 ⁇ m or less was regarded as acceptable, and a ceramic sintered body having a maximum pore diameter of 10 ⁇ m or more was regarded as rejected.
  • Examples 8 to 10 are reference examples, and it can be seen that by performing the CIP treatment, a dense and high-strength ceramic sintered body can be produced even by a two-step heat treatment.
  • Examples 11 to 18 are comparative examples, and it can be seen that a dense and high-strength ceramic sintered body cannot be produced when the CIP treatment is not performed and the two-step heat treatment is performed.
  • Examples 1 to 5, 19 and 20 are examples, and it can be seen that a dense and high-strength ceramic sintered body can be produced by performing a three-step heat treatment without performing the CIP treatment.
  • Examples 6 and 7 are also examples, and it was found that a dense and high-strength ceramic sintered body can be produced by performing a three-step heat treatment after the CIP treatment, and further, when the CIP treatment is not performed. In comparison, it can be seen that the number and size of the pores are smaller.
  • Example 2 Example 2 in which the fracture toughness value of the ceramic sintered body is evaluated will be described.
  • Examples 21, 22 and 24 are examples, and examples 23 and 25 are comparative examples.
  • Table 2 shows the production conditions of the ceramic sintered body according to each example.
  • Table 3 shows the evaluation results of the ceramic sintered body according to each example.
  • 4 and 5 are graphs showing fracture toughness values in Example 2.
  • FIG. 4 shows the fracture toughness value for each distance from the surface with respect to the radius r
  • FIG. 5 shows the fracture toughness value for each distance (absolute value) from the surface.
  • Example 21 As an example 21, a spherical silicon nitride ceramics sintered body was manufactured. The diameter obtained was 51 mm. In Example 21, a spherical molding die (diameter 64 mm) was used as the molding die, and a spherical silicon nitride sintered body was obtained as the ceramics sintered body.
  • the conditions different from Example 1 are as follows. The Sp amount was 4 mol%, and the heat treatment under the first conditions was carried out at 1400 ° C. for 5 hours to obtain a first sintered body. As a heat treatment under the second condition, the first sintered body was heat-treated at 1800 ° C.
  • a ceramic sintered body (silicon nitride sintered body) was produced by the same method as in Example 1 except for the above points.
  • the obtained ceramic sintered body was measured fracture toughness value (K IC) and Vickers hardness.
  • K IC was cut into a disk having a thickness of 10 mm so as to pass through the diameter of the obtained ceramic sintered body, and then one of the cut surfaces was polished to measure the K IC along the radial direction of the sphere.
  • Example 22 the ceramic sintered body was produced by the same method as in Example 21 except that the size of the molding die was 63 mm in diameter and the heat treatment under the first condition was performed at 1600 ° C. for 5 hours. The diameter of the obtained ceramic sintered body was 50 mm.
  • Example 23 the ceramic sintered body was produced by the same method as in Example 21 except that the heat treatment under the first condition was not performed.
  • the diameter was 51 mm.
  • Example 24 the ceramic sintered body was produced by the same method as in Example 21 except that the size of the spherical molding was 15 mm in diameter and the heat treatment under the first condition was performed at 1600 ° C. for 3.5 hours. The diameter of the obtained ceramic sintered body was 12 mm.
  • Example 25 a ceramic sintered body was produced by the same method as in Example 17, except that the CIP-treated molded product was processed to a diameter of 60.8 mm. The diameter was 50 mm.
  • Example 21 As shown in Table 3, in the example 21, 22, 24 is an example, K IC in the region from the surface to a depth r / 10, ⁇ KA, ⁇ KB, respectively, 6.5, 2.0 , 1.5 or less, and it can be seen that the density is improved and the abrasion resistance is improved.
  • Example 23 is a comparative example, in Example 25, K IC in the region from the surface to a depth r / 10, ⁇ KA, at least one ⁇ KB but is outside the above range, that wear resistance can not be improved I understand.
  • the embodiments and examples of the present invention have been described above, the embodiments are not limited by the contents of the embodiments and the examples. Further, the above-mentioned components include those that can be easily assumed by those skilled in the art, those that are substantially the same, that is, those in a so-called equal range. Furthermore, the components described above can be combined as appropriate. Further, various omissions, replacements or changes of the components can be made without departing from the gist of the above-described embodiment.

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Abstract

Dans la présente invention, un corps fritté en céramique dense est produit de manière appropriée. Un procédé de production d'un corps fritté en céramique selon la présente invention comprend : une étape de traitement thermique, sous une première condition, d'un corps moulé en céramique qui est un corps moulé en poudre de céramique ; une étape de traitement thermique, sous une deuxième condition dans laquelle la pression est supérieure à la pression de la première condition, du corps moulé en céramique qui a été traité thermiquement sous la première condition ; et une étape de production d'un corps fritté en céramique par traitement thermique, sous une troisième condition dans laquelle la pression est supérieure à la pression de la deuxième condition, du corps moulé en céramique qui a été traité thermiquement dans la deuxième condition.
PCT/JP2021/017471 2020-05-07 2021-05-07 Procédé de production de corps fritté en céramique, et corps fritté en céramique Ceased WO2021225158A1 (fr)

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WO2023145672A1 (fr) * 2022-01-27 2023-08-03 Ntn株式会社 Corps fritté de nitrure de silicium, élément de machine mettant en œuvre un tel corps fritté et palier
JP2023109655A (ja) * 2022-01-27 2023-08-08 Ntn株式会社 窒化ケイ素焼結体、それを用いた機械部品、および軸受
JP2023127845A (ja) * 2022-03-02 2023-09-14 Ntn株式会社 窒化ケイ素素球、転動体、および転がり軸受
WO2024019143A1 (fr) * 2022-07-22 2024-01-25 Ａｇｃ株式会社 Corps fritté en nitrure de silicium et procédé de fabrication d'un corps fritté en nitrure de silicium
WO2024043230A1 (fr) * 2022-08-24 2024-02-29 Ａｇｃ株式会社 Corps fritté en nitrure de silicium et procédé de fabrication de corps fritté en nitrure de silicium

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CN114044682A (zh) * 2021-11-29 2022-02-15 上海材料研究所 一种水基浆料凝胶注模成型制备高导热氮化硅陶瓷的方法
WO2023145672A1 (fr) * 2022-01-27 2023-08-03 Ntn株式会社 Corps fritté de nitrure de silicium, élément de machine mettant en œuvre un tel corps fritté et palier
JP2023109655A (ja) * 2022-01-27 2023-08-08 Ntn株式会社 窒化ケイ素焼結体、それを用いた機械部品、および軸受
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WO2024043230A1 (fr) * 2022-08-24 2024-02-29 Ａｇｃ株式会社 Corps fritté en nitrure de silicium et procédé de fabrication de corps fritté en nitrure de silicium

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